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CAS No. : | 1173047-86-3 | MDL No. : | MFCD11505546 |
Formula : | C9H13BrClN | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | KMJLJHXKDTUCRP-UHFFFAOYSA-N |
M.W : | 250.56 | Pubchem ID : | 42956122 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
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* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
11.4 g | With triethylamine; In dichloromethane; at 20℃; for 18h; | Step 1: tert-butyl (2-(4-bromophenyl)propan-2-yl)carbamate: A solution of 2- (4- bromophenyl)propan-2-amine hydrochloride (10 g, 39.9 mmol) and Et3N (5.84 ml, 41.9 mmol) in DCM (100 ml) was treated with Boc20 (9.15 g, 41.9 mmol) and stirred at RT for 18 h. The reaction mixture was washed with a saturated NH4Cl(aq) (100 ml) and the organic phase was concentrated in vacuo. The residue was purified by columnchromatography (220 g cartridge, 0-30% EtOAc/isohexane) to afford the title compound (11.4 g, 35.0 mmol, 97% purity) as a flocculent white solid. LCMS (Method 1): m/z 258 (M+H-C4H8)+ at 2.64 min. |
With triethylamine; In dichloromethane; at 0 - 20℃; | Preparation 249: tert-butyl (2-(4-bromophenyl)propan-2-yl)carbamate (1920) ==/ NHBoc (1921) Boc-anhydride (278 muIota, 1.197 mmol) and triethylamine (306 muIota, 2.195 mmol) were added to a solution of 2-(4-bromophenyl)propan-2-amine.HCI (250 mg, 0.998 mmol) in DCM (10 ml_) at 0 C. The reaction mixture was allowed to warm to room temperature and stirred overnight. The reaction mixture was washed with 1 M HCI (aq.) (5 ml_), and brine (5 ml_), dried (Na2S04), filtered and concentrated in vacuo to afford the title compound (332 mg, 101 %) as a colourless oil which solidified on standing. 1 H NMR (Chloroform-d) delta: 7.47 - 7.38 (m, 2H), 7.31 - 7.22 (m, 2H), 4.91 (s, 1 H), 1.59 (s, 6H), 1.52 (d, 9H). |
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